CN106928510A - A kind of oil-resisting and heat-resisting elastomeric material and preparation method thereof - Google Patents
A kind of oil-resisting and heat-resisting elastomeric material and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
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- C08L9/00—Compositions of homopolymers or copolymers of conjugated diene hydrocarbons
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Abstract
The invention provides a kind of oil-resisting and heat-resisting elastomeric material and preparation method thereof.Preparation method is as follows：（1）Prepare modified sodium hexatitanate whisker；（2）Following component is weighed by weight：70 100 parts of nitrile rubber, 30 50 parts of silicon rubber, 47 parts of zinc oxide, 20 40 parts of carbon black, 24 parts of glycerine, 0.5 2.5 parts of zinc stearate, 5 12 parts of dioctyl phthalate, 24 parts of sulphur, captax are 0.5 1.5 parts, TM monex TM is 0.5 1 parts, antioxidant 4010NA is 0.5 1.5 parts, antioxidant A W is 0.5 1.2 parts, 26 parts of 2 ethyl acetic acid zirconium, 2.5 5 parts of trimethyl silicane potassium alcoholate, modified 37 parts of sodium hexatitanate whisker；（3）By banburying, then knead, vulcanization is obtained elastomeric material.Oil-resisting and heat-resisting elastomeric material formula of the invention is reasonable, process is simple, with good heat-resisting oil resistance.
Description
Technical field
The present invention relates to field of rubber materials, and in particular to a kind of oil-resisting and heat-resisting elastomeric material and preparation method thereof.
Background technology
Nitrile rubber has high steady to nonpolar or low pole mineral oil, vegetable and animals oils, liquid fuel and solvent etc.
It is qualitative, therefore nitrile rubber is often used in the rubbers such as manufacture oil-resisting rubber hose, oil-resistant seal ring, oil service conveyor belt.And with
The development of oil and auto industry, more harsh requirement is proposed to nitrile rubber, promote the research of nitrile rubber.Silicon rubber
Glue is set with its excellent weatherability, resistant of high or low temperature, electrical insulating property, radiation resistance, biologically inert etc. in electric, electronics, office
The fields such as standby, automobile, building, medical treatment, food and man-made organ have a wide range of applications.Silicon rubber is in the range of -60-200 DEG C
Can long-term use.With the development of modern science and technology, the requirement more and more higher to silicon rubber heat-resisting.Such as the hair of high speed car
Motivation cabin temperature often more than 300 DEG C, oil resistant higher, high temperature resistant requirement is proposed to rubber accessory.Therefore, development is carried
The elastomeric material of high nitrile rubber, the research of silicon rubber heat endurance, manufacture with more operation at high temperature has practical significance.State
It is inside and outside that many research is had been carried out with regard to heat-resisting resistance oil silicone rubber.The heat-resisting group of large volume is introduced such as in main chain or is changed
The structure for becoming side chain can also improve rubber heat resistance, and these method costs are all higher, operate more complicated.
The content of the invention
The technical problem to be solved：It is an object of the invention to provide a kind of oil-resisting and heat-resisting elastomeric material, preparation process is simple,
Possess preferable oil resistivity and heat resistance.
Technical scheme：A kind of preparation method of oil-resisting and heat-resisting elastomeric material, comprises the following steps：
（1）By sodium hexatitanate whisker be configured to concentration be 10-18wt% the aqueous solution, be uniformly dispersed, heating water bath to 75 DEG C, so
It is the sodium silicate solution of 3-6wt% to add concentration afterwards, is incubated 5h, and filtration washing obtains coated Si O after drying2Sodium hexatitanate it is brilliant
Palpus；
（2）By Silane coupling reagent KH-570 and coated Si O2Sodium hexatitanate whisker add concentration be 80-95wt% ethanol solutions
In, the mass ratio of three is 3:100:500, ultrasonic disperse 5-15min, stir 20-35min at 70 DEG C of constant temperature, filtering is cleaned dry
The dry sodium hexatitanate whisker that must be modified；
（3）Following component is weighed by weight：Nitrile rubber 70-100 parts, silicon rubber 30-50 parts, zinc oxide 4-7 parts, carbon black
20-40 parts, glycerine 2-4 parts, zinc stearate 0.5-2.5 parts, dioctyl phthalate 5-12 parts, sulphur 2-4 parts, accelerator
M is 0.5-1.5 parts, TM monex TM is 0.5-1 parts, antioxidant 4010NA is 0.5-1.5 parts, antioxidant A W is 0.5-1.2 parts,
2-6 parts of 2- ethyl acetic acid zirconiums, 2.5-5 parts of trimethyl silicane potassium alcoholate, modified 3-7 parts of sodium hexatitanate whisker；
（4）In banbury, nitrile rubber, silicon rubber are added, in 105-115 DEG C of temperature in banburying 3-5min, be subsequently adding oxygen
Change zinc, carbon black, glycerine, zinc stearate, dioctyl phthalate, sulphur, captax, TM monex TM, age resistor
4010NA, antioxidant A W, 2- ethyl acetic acid zirconium, trimethyl silicane potassium alcoholate, modified sodium hexatitanate whisker, enter at being cooled to 80-90 DEG C
Row mixing 4-6min, the compression molding in vulcanizing press by blend, temperature is vulcanization under the conditions of 160-200 DEG C.
Further, a kind of preparation method of described oil-resisting and heat-resisting elastomeric material, the step（1）Middle sodium hexatitanate is brilliant
Palpus concentration of aqueous solution is 15wt%, and sodium silicate solution concentration is 4.5%.
Further, a kind of preparation method of described oil-resisting and heat-resisting elastomeric material, the step（2）Middle concentration of alcohol is
85-90wt%, the ultrasonic disperse time is 10min, and mixing time is 25-30min.
Further, a kind of preparation method of described oil-resisting and heat-resisting elastomeric material, the step（3）In claim by weight
Take following component：Nitrile rubber 80-90 parts, silicon rubber 35-45 parts, zinc oxide 5-6 parts, carbon black 25-35 parts, glycerine 3-4 parts,
Zinc stearate 1-2 parts, dioctyl phthalate 6-10 parts, sulphur 2-3 parts, captax be 0.7-1.2 parts, TM monex TM
For 0.6-0.8 parts, antioxidant 4010NA be 0.8-1.2 part, antioxidant A W be 0.8-1 parts, 3-5 parts of 2- ethyl acetic acid zirconiums, front three
3-4 parts of base silanol potassium, modified 4-6 parts of sodium hexatitanate whisker.
Further, a kind of preparation method of described oil-resisting and heat-resisting elastomeric material, the step（4）Middle mixing temperature is
110 DEG C, mixing time is 4min, and melting temperature is 85 DEG C, and mixing time is 5min, and curing temperature is 180 DEG C.
A kind of above-mentioned oil-resisting and heat-resisting elastomeric material, preparation side of the oil-resisting and heat-resisting elastomeric material as described in any of the above-described
Method is prepared from.
Beneficial effect：Oil-resisting and heat-resisting elastomeric material of the invention contains 2- ethyl acetic acids zirconium, trimethyl silicane potassium alcoholate, modified six
Sodium titanate crystal whisker, the oil resistivity of the rubber produced with this rubber compounding is less than 6.1%, and heat ageing coefficient is high, and stable performance is resistance to
Hot good, sealing property is good.
Specific embodiment
Embodiment 1
A kind of preparation method of oil-resisting and heat-resisting elastomeric material, comprises the following steps：（1）Sodium hexatitanate whisker is configured into concentration is
The aqueous solution of 10wt%, is uniformly dispersed, and heating water bath is subsequently adding the sodium silicate solution that concentration is 6wt% to 75 DEG C, is incubated 5h,
Filtration washing obtains coated Si O after drying2Sodium hexatitanate whisker；（2）By Silane coupling reagent KH-570 and coated Si O2Six titaniums
Sour sodium whisker adds concentration in 80wt% ethanol solutions, the mass ratio of three is 3:100:500, ultrasonic disperse 15min, constant temperature
Stir 20min at 70 DEG C, filtering clean dry must be modified sodium hexatitanate whisker；（3）Following component is weighed by weight：Butyronitrile rubber
70 parts of glue, 50 parts of silicon rubber, 4 parts of zinc oxide, 20 parts of carbon black, 4 parts of glycerine, 0.5 part of zinc stearate, dioctyl phthalate
5 parts, 2 parts of sulphur, captax be 0.5 part, TM monex TM be 1 part, antioxidant 4010NA be 0.5 part, antioxidant A W be 1.2
Part, 2 parts of 2- ethyl acetic acids zirconium, 5 parts of trimethyl silicane potassium alcoholate, modified 3 parts of sodium hexatitanate whisker；（4）In banbury, butyronitrile is added
Rubber, silicon rubber, in 105 DEG C of temperature in banburying 3-5min, are subsequently adding zinc oxide, carbon black, glycerine, zinc stearate, adjacent benzene
Diformazan dioctyl phthalate, sulphur, captax, TM monex TM, antioxidant 4010NA, antioxidant A W, 2- ethyl acetic acid zirconium, front three
Base silanol potassium, modified sodium hexatitanate whisker, mixing 4min is carried out at being cooled to 80 DEG C, and blend is molded in vulcanizing press
Shaping, temperature is vulcanization under the conditions of 160 DEG C.
Embodiment 2
A kind of preparation method of oil-resisting and heat-resisting elastomeric material, comprises the following steps：（1）Sodium hexatitanate whisker is configured into concentration is
The aqueous solution of 18wt%, is uniformly dispersed, and heating water bath is subsequently adding the sodium silicate solution that concentration is 3wt% to 75 DEG C, is incubated 5h,
Filtration washing obtains coated Si O after drying2Sodium hexatitanate whisker；（2）By Silane coupling reagent KH-570 and coated Si O2Six titaniums
Sour sodium whisker adds concentration in 95wt% ethanol solutions, the mass ratio of three is 3:100:500, ultrasonic disperse 5min, constant temperature 70
Stir 35min at DEG C, filtering clean dry must be modified sodium hexatitanate whisker；（3）Following component is weighed by weight：Nitrile rubber
100 parts, 30 parts of silicon rubber, 7 parts of zinc oxide, 40 parts of carbon black, 2 parts of glycerine, 2.5 parts of zinc stearate, dioctyl phthalate
12 parts, 4 parts of sulphur, captax be 1.5 parts, TM monex TM be 0.5 part, antioxidant 4010NA be 1.5 parts, antioxidant A W be
0.5 part, 6 parts of 2- ethyl acetic acids zirconium, 2.5 parts of trimethyl silicane potassium alcoholate, modified 7 parts of sodium hexatitanate whisker；（4）In banbury, plus
Enter nitrile rubber, silicon rubber, in 115 DEG C of temperature in banburying 3-5min, be subsequently adding zinc oxide, carbon black, glycerine, stearic acid
Zinc, dioctyl phthalate, sulphur, captax, TM monex TM, antioxidant 4010NA, antioxidant A W, 2- ethyl acetic acid
Zirconium, trimethyl silicane potassium alcoholate, modified sodium hexatitanate whisker, carry out mixing 6min, by blend in compression molding at being cooled to 90 DEG C
Compression molding in machine, temperature is vulcanization under the conditions of 200 DEG C.
Embodiment 3
A kind of preparation method of oil-resisting and heat-resisting elastomeric material, comprises the following steps：（1）Sodium hexatitanate whisker is configured into concentration is
The aqueous solution of 15wt%, is uniformly dispersed, and heating water bath is subsequently adding the sodium silicate solution that concentration is 4.5wt%, insulation to 75 DEG C
5h, filtration washing obtains coated Si O after drying2Sodium hexatitanate whisker；（2）By Silane coupling reagent KH-570 and coated Si O2's
Sodium hexatitanate whisker adds concentration in 85wt% ethanol solutions, the mass ratio of three is 3:100:500, ultrasonic disperse 10min,
Stir 25min at 70 DEG C of constant temperature, filtering clean dry must be modified sodium hexatitanate whisker；（3）Following component is weighed by weight：Fourth
80 parts of nitrile rubber, 45 parts of silicon rubber, 6 parts of zinc oxide, 25 parts of carbon black, 4 parts of glycerine, 2 parts of zinc stearate, phthalic acid two are pungent
6 parts of ester, 2 parts of sulphur, captax are 0.7 part, TM monex TM is 0.8 part, antioxidant 4010NA is 1.2 parts, antioxidant A W is
1 part, 3 parts of 2- ethyl acetic acids zirconium, 4 parts of trimethyl silicane potassium alcoholate, modified 4 parts of sodium hexatitanate whisker；（4）In banbury, fourth is added
Nitrile rubber, silicon rubber, in 110 DEG C of temperature in banburying 4min, are subsequently adding zinc oxide, carbon black, glycerine, zinc stearate, adjacent benzene
Diformazan dioctyl phthalate, sulphur, captax, TM monex TM, antioxidant 4010NA, antioxidant A W, 2- ethyl acetic acid zirconium, front three
Base silanol potassium, modified sodium hexatitanate whisker, mixing 5min is carried out at being cooled to 85 DEG C, and blend is molded in vulcanizing press
Shaping, temperature is vulcanization under the conditions of 180 DEG C.
Embodiment 4
A kind of preparation method of oil-resisting and heat-resisting elastomeric material, comprises the following steps：（1）Sodium hexatitanate whisker is configured into concentration is
The aqueous solution of 15wt%, is uniformly dispersed, and heating water bath is subsequently adding the sodium silicate solution that concentration is 4.5wt%, insulation to 75 DEG C
5h, filtration washing obtains coated Si O after drying2Sodium hexatitanate whisker；（2）By Silane coupling reagent KH-570 and coated Si O2's
Sodium hexatitanate whisker adds concentration in 90wt% ethanol solutions, the mass ratio of three is 3:100:500, ultrasonic disperse 10min,
Stir 30min at 70 DEG C of constant temperature, filtering clean dry must be modified sodium hexatitanate whisker；（3）Following component is weighed by weight：Fourth
90 parts of nitrile rubber, 35 parts of silicon rubber, 5 parts of zinc oxide, 35 parts of carbon black, 3 parts of glycerine, 1 part of zinc stearate, phthalic acid two are pungent
10 parts of ester, 3 parts of sulphur, captax are 1.2 parts, TM monex TM is 0.6 part, antioxidant 4010NA is 0.8 part, antioxidant A W
For 0.8 part, 5 parts of 2- ethyl acetic acids zirconium, 3 parts of trimethyl silicane potassium alcoholate, modified 6 parts of sodium hexatitanate whisker；（4）In banbury, plus
Enter nitrile rubber, silicon rubber, in 110 DEG C of temperature in banburying 4min, be subsequently adding zinc oxide, carbon black, glycerine, zinc stearate,
Dioctyl phthalate, sulphur, captax, TM monex TM, antioxidant 4010NA, antioxidant A W, 2- ethyl acetic acid zirconium,
Trimethyl silicane potassium alcoholate, modified sodium hexatitanate whisker, carry out mixing 5min, by blend in vulcanizing press at being cooled to 85 DEG C
Compression molding, temperature is vulcanization under the conditions of 180 DEG C.
Embodiment 5
A kind of preparation method of oil-resisting and heat-resisting elastomeric material, comprises the following steps：（1）Sodium hexatitanate whisker is configured into concentration is
The aqueous solution of 15wt%, is uniformly dispersed, and heating water bath is subsequently adding the sodium silicate solution that concentration is 4.5wt%, insulation to 75 DEG C
5h, filtration washing obtains coated Si O after drying2Sodium hexatitanate whisker；（2）By Silane coupling reagent KH-570 and coated Si O2's
Sodium hexatitanate whisker adds concentration in 88wt% ethanol solutions, the mass ratio of three is 3:100:500, ultrasonic disperse 10min,
Stir 26min at 70 DEG C of constant temperature, filtering clean dry must be modified sodium hexatitanate whisker；（3）Following component is weighed by weight：Fourth
85 parts of nitrile rubber, 40 parts of silicon rubber, 5 parts of zinc oxide, 30 parts of carbon black, 3 parts of glycerine, 1.5 parts of zinc stearate, phthalic acid two
8 parts of monooctyl ester, 2.4 parts of sulphur, captax are 1 part, TM monex TM is 0.7 part, antioxidant 4010NA is 1 part, antioxidant A W is
0.9 part, 4 parts of 2- ethyl acetic acids zirconium, 4 parts of trimethyl silicane potassium alcoholate, modified 5 parts of sodium hexatitanate whisker；（4）In banbury, add
Nitrile rubber, silicon rubber, in 110 DEG C of temperature in banburying 4min, are subsequently adding zinc oxide, carbon black, glycerine, zinc stearate, neighbour
Dioctyl phthalate, sulphur, captax, TM monex TM, antioxidant 4010NA, antioxidant A W, 2- ethyl acetic acid zirconium, three
Methyl silanol potassium, modified sodium hexatitanate whisker, mixing 5min is carried out at being cooled to 85 DEG C, by blend in vulcanizing press mould
Molded, temperature is vulcanization under the conditions of 180 DEG C.
Comparative example 1
A kind of preparation method of oil-resisting and heat-resisting elastomeric material, comprises the following steps：（1）Following component is weighed by weight：Butyronitrile
70 parts of rubber, 50 parts of silicon rubber, 4 parts of zinc oxide, 20 parts of carbon black, 4 parts of glycerine, 0.5 part of zinc stearate, phthalic acid two are pungent
5 parts of ester, 2 parts of sulphur, captax are 0.5 part, TM monex TM is 1 part, antioxidant 4010NA is 0.5 part, antioxidant A W is
1.2 parts, 2 parts of 2- ethyl acetic acids zirconium, 5 parts of trimethyl silicane potassium alcoholate, 3 parts of sodium hexatitanate whisker；（2）In banbury, butyronitrile is added
Rubber, silicon rubber, in 105 DEG C of temperature in banburying 3-5min, are subsequently adding zinc oxide, carbon black, glycerine, zinc stearate, adjacent benzene
Diformazan dioctyl phthalate, sulphur, captax, TM monex TM, antioxidant 4010NA, antioxidant A W, 2- ethyl acetic acid zirconium, front three
Base silanol potassium, modified sodium hexatitanate whisker, mixing 4min is carried out at being cooled to 80 DEG C, and blend is molded in vulcanizing press
Shaping, temperature is vulcanization under the conditions of 160 DEG C.
Comparative example 2
A kind of preparation method of oil-resisting and heat-resisting elastomeric material, comprises the following steps：（1）Sodium hexatitanate whisker is configured into concentration is
The aqueous solution of 18wt%, is uniformly dispersed, and heating water bath is subsequently adding the sodium silicate solution that concentration is 3wt% to 75 DEG C, is incubated 5h,
Filtration washing obtains coated Si O after drying2Sodium hexatitanate whisker；（2）By Silane coupling reagent KH-570 and coated Si O2Six titaniums
Sour sodium whisker adds concentration in 95wt% ethanol solutions, the mass ratio of three is 3:100:500, ultrasonic disperse 5min, constant temperature 70
Stir 35min at DEG C, filtering clean dry must be modified sodium hexatitanate whisker；（3）Following component is weighed by weight：Nitrile rubber
100 parts, 30 parts of silicon rubber, 7 parts of zinc oxide, 40 parts of carbon black, 2 parts of glycerine, 2.5 parts of zinc stearate, dioctyl phthalate
12 parts, 4 parts of sulphur, captax be 1.5 parts, TM monex TM be 0.5 part, antioxidant 4010NA be 1.5 parts, antioxidant A W be
0.5 part, modified 7 parts of sodium hexatitanate whisker；（4）In banbury, nitrile rubber, silicon rubber are added, in 115 DEG C of temperature in banburying
3-5min, is subsequently adding zinc oxide, carbon black, glycerine, zinc stearate, dioctyl phthalate, sulphur, captax, promotion
Agent TMTM, antioxidant 4010NA, antioxidant A W, modified sodium hexatitanate whisker, mixing 6min is carried out at being cooled to 90 DEG C, will be blended
Thing compression molding in vulcanizing press, temperature is vulcanization under the conditions of 200 DEG C.
The property indices of material of the present invention see the table below, it may be seen that containing 2- in this oil-resisting and heat-resisting elastomeric material
Ethyl acetic acid zirconium, trimethyl silicane potassium alcoholate, modified sodium hexatitanate whisker, the oil resistivity of the rubber produced with this rubber compounding are less than
6.1%, heat ageing coefficient is high, and stable performance is heat-resist, and sealing property is good.
The property indices of the oil-resisting and heat-resisting elastomeric material of table 1
Claims (6)
1. a kind of preparation method of oil-resisting and heat-resisting elastomeric material, it is characterised in that comprise the following steps：
（1）By sodium hexatitanate whisker be configured to concentration be 10-18wt% the aqueous solution, be uniformly dispersed, heating water bath to 75 DEG C, so
It is the sodium silicate solution of 3-6wt% to add concentration afterwards, is incubated 5h, and filtration washing obtains coated Si O after drying2Sodium hexatitanate it is brilliant
Palpus；
（2）By Silane coupling reagent KH-570 and coated Si O2Sodium hexatitanate whisker add concentration be 80-95wt% ethanol solutions in,
The mass ratio of three is 3:100:500, ultrasonic disperse 5-15min, stir 20-35min at 70 DEG C of constant temperature, filtering clean dry is obtained
Modified sodium hexatitanate whisker；
（3）Following component is weighed by weight：Nitrile rubber 70-100 parts, silicon rubber 30-50 parts, zinc oxide 4-7 parts, carbon black
20-40 parts, glycerine 2-4 parts, zinc stearate 0.5-2.5 parts, dioctyl phthalate 5-12 parts, sulphur 2-4 parts, accelerator
M is 0.5-1.5 parts, TM monex TM is 0.5-1 parts, antioxidant 4010NA is 0.5-1.5 parts, antioxidant A W is 0.5-1.2 parts,
2-6 parts of 2- ethyl acetic acid zirconiums, 2.5-5 parts of trimethyl silicane potassium alcoholate, modified 3-7 parts of sodium hexatitanate whisker；
（4）In banbury, nitrile rubber, silicon rubber are added, in 105-115 DEG C of temperature in banburying 3-5min, be subsequently adding oxygen
Change zinc, carbon black, glycerine, zinc stearate, dioctyl phthalate, sulphur, captax, TM monex TM, age resistor
4010NA, antioxidant A W, 2- ethyl acetic acid zirconium, trimethyl silicane potassium alcoholate, modified sodium hexatitanate whisker, enter at being cooled to 80-90 DEG C
Row mixing 4-6min, the compression molding in vulcanizing press by blend, temperature is vulcanization under the conditions of 160-200 DEG C.
2. the preparation method of a kind of oil-resisting and heat-resisting elastomeric material according to claim 1, it is characterised in that：The step
（1）Middle sodium hexatitanate whisker concentration of aqueous solution is 15wt%, and sodium silicate solution concentration is 4.5%.
3. the preparation method of a kind of oil-resisting and heat-resisting elastomeric material according to claim 1, it is characterised in that：The step
（2）Middle concentration of alcohol is 85-90wt%, and the ultrasonic disperse time is 10min, and mixing time is 25-30min.
4. the preparation method of a kind of oil-resisting and heat-resisting elastomeric material according to claim 1, it is characterised in that：The step
（3）In weigh following component by weight：Nitrile rubber 80-90 parts, silicon rubber 35-45 parts, zinc oxide 5-6 parts, carbon black 25-35
Part, glycerine 3-4 part, zinc stearate 1-2 parts, dioctyl phthalate 6-10 parts, sulphur 2-3 parts, captax be 0.7-
1.2 parts, TM monex TM be 0.6-0.8 part, antioxidant 4010NA be 0.8-1.2 parts, antioxidant A W be 0.8-1 parts, 2- ethyls
Zirconium acetate 3-5 parts, 3-4 parts of trimethyl silicane potassium alcoholate, modified 4-6 parts of sodium hexatitanate whisker.
5. the preparation method of a kind of oil-resisting and heat-resisting elastomeric material according to claim 1, it is characterised in that：The step
（4）Middle mixing temperature is 110 DEG C, and mixing time is 4min, and melting temperature is 85 DEG C, and mixing time is 5min, and curing temperature is
180℃。
6. a kind of oil-resisting and heat-resisting elastomeric material, its special medical treatment is：The oil-resisting and heat-resisting elastomeric material is by claim any one of 1-5
Described preparation method is prepared from.
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| CN110144121A (en) * | 2019-05-21 | 2019-08-20 | 于世强 | A kind of oil pumping cabinet carbon silicone oil envelope |
| CN111117013A (en) * | 2019-12-29 | 2020-05-08 | 河北新尔特橡塑密封有限公司 | Heat-resistant oil-resistant sealing ring and preparation method thereof |
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